GC-MS测定PU革中3种有机磷阻燃剂

GC-MS determination of three organophosphorous flame retardants in PU leather

研究建立了GC-MS测定聚氨酯(PU)革中3种有机磷阻燃剂三(2-氯乙基)磷酸酯、三(2-氯丙基)磷酸酯三和(1,3-二氯异丙基)磷酸酯的分析方法。室温条件下,以四氢呋喃∶正己烷(1∶1)为溶剂超声溶解PU革30min,萃取液通过气相色谱/质谱-选择离子监测法进行定量分析。3种有机磷阻燃剂的线性范围为0.3mg/kg^10mg/kg;相关系数大于0.995;方法检测限范围为0.04~0.09mg/kg;平均回收率在89.9%~109.2%,相对标准偏差(n=6)小于10%。该方法简便快速、灵敏度高、定性准确,满足PU革中有机磷阻燃剂的检测要求。

Three organophosphorous flame retardants from polyurethane （PU） leather were tris （2- chloroethyl） phosphate and tris（2-chloro-isopropyl） phosphate, tris（1,3-dichloro-isopropyl）phosphate. At room temperature, the sample was dissolved by tetrahydrofuran and hexane （1 ： 1） with ultrasonic extraction for 30 min, and then the extracts were analyzed by GC-MS with selected ion monitor technique. The calibration curves of three kinds of organophosphorous flame retardants were linear in the range of 0.3- 10mg/kg, with the correlation coefficients better than 0. 995. The detection limit were in the range of 0.04 -0.09 mg/kg, the average recoveries ranged from 89.9% to 109.2%, and the relative standard deviations （n= 6） were less than 10%. The results showed that this method was simple, rapid, sensitive and accurate.